液相色谱法测定奶粉中三聚氰胺的方法优化

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1、※分析检测食品科学2009,Vol.30,No.14227液相色谱法测定奶粉中三聚氰胺的方法优化李燕，柴勇，龚久平，刘吉振*，易志坚，洪云菊，高静(农业部农产品质量安全监督检验测试中心(重庆)，重庆市农业科学院农业质量标准检测技术研究所，重庆400055)摘要：优化了反相高效液相色谱测定奶粉中三聚氰胺的方法。样品制备：采用乙酸铅对奶粉中的蛋白质进行沉淀，用1%的三氯乙酸代替水对阳离子交换固相萃取柱进行活化和洗涤；色谱条件：提高缓冲离子对试剂pH值为3.0，增加流动相中乙腈比例。结果：用外标法定量分析，标准曲线的相关系数为0.9997，

2、平均回收率为95.8%～101.5%。证明优化后的方法具有较好的回收率和重现性，可以准确地测定奶粉中的三聚氰胺。关键词：三聚氰胺；液相色谱；奶粉；优化OptimizationofRP-HPLCDeterminationofMelamineinMilkPowderLIYan，CHAIYong，GONGJiu-ping，LIUJi-zhen*，YIZhi-jian，HONGYun-ju，GAOJing(ChongqingSupervisionandTestingCenterforAgriculturalProductsQualityand

3、Security,MinistryofAgriculture,InstitutionofAgriculturalQualityStandardandTestingTechnology,ChongqingAcademyofAgriculturalSciences,Chongqing400055,China)Abstract：TheRP-HPLCmethodfordeterminingmelamineinmilkpowderhasbeendeveloped.However,thedifferencesinchromatographyins

4、trumentandcolumnperformanceandstatusmayleadtotheoccurrenceofdisagreementamongdetermina-tionresultsfromdifferentlabs.Toenhancetheaccuracy,reproducibilityandefficiencyofmelaminedetectionbyHPLC,samplepreparationandchromatographicconditionswereoptimizedinthepresentstudy.Mil

5、kpowdersampleswereextractedusing1%trichloroaceticacidand2%leadacetatesolutioninanultrasonicfieldandcleaneduponanSCXsolidphaseextractioncolumnwhichwasactivatedandleachedusing1%trichloroaceticacidinsteadofwater.Theoptimizationofchromatographicconditionswasachievedbyincrea

6、singtheion-pairingbuffercontaining10mmolcitricacidand10mmolheptane-1-sulfonicacidsodiumsalttopH3andadjustingtheproportionofacetonitrileinthemobilephaseconsistingofitandtheion-pairingbufferto28%(V/V).Theexternalstandardmethodwasadoptedforthequantitativeanalysisofmelamine

7、.Thecorrelationcoefficientoflinearequationwas0.9997andthelimitofdetectionofmelaminewas0.15mg/kgbythismethod.Therecoveriesformelamineinblankmilkpowderspikedatfivelevelswerewithin95.8%－101.5%.Theoptimizedmethodhashighreproducibilityandallowsaccuratedetectionandhighrecover

8、yformelamineinmilkpowder.Keywords：melamine；HPLC；milkpowder；optimization中图分类号：TS207.53文献标识码：A文章编号：1002-6630(200